HRID601554

反应详情

EQUATION

反应方程式

HRID 601554 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Add lithium bromide (955 mg, 11.0 mmol) to a mixture of isobutylene oxide (6.20 mL, 68.8 mmol) and benzyl-(2-methyl-allyl)-amine (9.51 g, 59.0 mmol). Stir the mixture for 3.5 h at room temperature then treat with additional epoxide (1.5 mL, 16.6 mmol) and heat at 60° C. for 1.7 h. Dilute the mixture with CH2Cl2 (200 mL) and wash with water (200 mL). Dry, filter and concentrate the organic solution. Dry the residue at 80° C. under vacuum to give the title compound (13.5 g, 98%) as a colorless oil. 1H NMR (400 MHz, DMSO-d6): δ 7.2-7.4 (5H, m), 4.90 (1H, s), 4.83 (1H, s), 4.18 (1H, s), 3.59 (2H, s), 2.98 (2H, s), 2.27 (2H, s), 1.71 (3H, s), 1.05 (6H, s).

WORKUP

后处理

  1. temperatureheat at 60° C. for 1.7 h
  2. washwash with water (200 mL)
  3. customDry
  4. filtrationfilter
  5. concentrationconcentrate the organic solution
  6. customDry the residue at 80° C. under vacuum